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GB/T 18882.2-2017: Chemical analysis methods for mixed rare earth oxide of ion-absorbed type rare earth ore - Part 2: Determination of aluminum oxide content Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB/T 18882.2: Historical versions
Similar standardsGB/T 18882.2-2017: Chemical analysis methods for mixed rare earth oxide of ion-absorbed type rare earth ore - Part 2: Determination of aluminum oxide content---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GBT18882.2-2017 GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA ICS 77.120.99 H 14 Replacing GB/T 18882.2-2008 Chemical analysis methods for mixed rare earth oxide of ion-absorpted type rare earth ore - Part 2: Determination of aluminum oxide content ISSUED ON: OCTOBER 14, 2017 IMPLEMENTED ON: MAY 01, 2018 Issued by: General Administration of Quality Supervision, Inspection and Quarantine; Standardization Administration of the People’s Republic of China. Table of ContentsForeword ... 3 1 Scope ... 5 2 Method 1: Inductively coupled plasma atomic emission spectrometry (ICP-OES) .. 5 3 Method 2: Titration ... 9 Chemical analysis methods for mixed rare earth oxide of ion-absorpted type rare earth ore - Part 2: Determination of aluminum oxide content1 ScopeThis Part of GB/T 18882 specifies the determination method of aluminum oxide content in mixed rare earth oxide of ion-absorpted type rare earth ore. This Part applies to the determination of aluminum oxide content in mixed rare earth oxide of ion-absorpted type rare earth ore, including two methods: Method 1 Inductively coupled plasma atomic emission spectrometry and Method 2 Titration. The determination range of Method 1 (mass fraction): 0.10% ~ 5.00%, and the determination range of Method 2 (mass fraction): 4.00% ~ 15.00%.2 Method 1: Inductively coupled plasma atomic emissionspectrometry (ICP-OES) 2.1 Principle of the method Decompose the test sample by nitric acid and hydrofluoric acid; after the perchloric acid has smoked out, dissolve it in hydrochloric acid to make it clear; use approximate matrix matching to eliminate the rare earth matrix interference; directly excite by argon plasma light source; perform the spectrum measurement. 2.2 Reagents and materials Unless otherwise specified, all reagents used in this Part are analytical reagents that meet national or industry standards, and the water used is grade-II water. 2.2.1 Hydrochloric acid (ρ = 1.19 g/mL). 2.2.2 Hydrofluoric acid (ρ = 1.13 g/mL). 2.2.3 Perchloric acid (ρ = 1.67 g/mL). 2.2.4 Nitric acid (ρ = 1.42 g/mL). 2.2.5 Hydrogen peroxide (30%). 2.2.6 Nitric acid (1+1). 2.3 Instruments and equipment 2.3.1 Inductively coupled plasma atomic emission spectrometer, resolution < 0.006 nm (at 200 nm). 2.3.2 Light source: argon plasma light source. 2.4 Test sample 2.4.1 The particle size of the test sample is less than 0.074 mm. 2.4.2 Pre-dry the sample at 105 ℃ ~ 110 ℃ for 2 h; then, place it in a desiccator to cool to room temperature. 2.5 Procedure 2.5.1 Test material Weigh 0.1g of test sample (2.4), accurate to 0.000 1 g. 2.5.2 Number of determinations Independently perform two determinations; take the average value. 2.5.3 Blank test Carry out a blank test together with the test material (2.5.1). 2.5.4 Preparation of analytical solution Place the test materials (2.5.1) in a 150 mL polytetrafluoroethylene beaker; add a small amount of water; add 2 mL of nitric acid (2.2.6); heat to decompose for 3 min ~ 5 min; add 2 mL of hydrofluoric acid (2.2.2) and continue to decompose for 3 min ~ 5 min; add 3 mL of perchloric acid (2.2.3) to smoke and evaporate to nearly dry; remove and cool slightly; add 10 mL of hydrochloric acid (2.2.7) and add 3 ~ 5 drops of hydrogen peroxide (2.2.5); heat to dissolve until clear; transfer the test solution into a 100 mL volumetric flask; use water to dilute to the mark; mix well; test. 2.5.5 Series standard configuration According to Table 2, transfer the standard stock solution into six 100 mL volumetric flasks; use water to dilute to the mark; mix well; test. Unless otherwise specified, all reagents used in this Part are analytical reagents that meet national or industry standards, and the water used is grade-II water. 3.2.1 Hydrochloric acid (ρ = 1.19 g/mL). 3.2.2 Hydrofluoric acid (ρ = 1.13 g/mL). 3.2.3 Hydrogen peroxide (30%). 3.2.4 Perchloric acid (ρ = 1.67 g/mL). 3.2.5 Nitric acid (ρ = 1.42 g/mL). 3.2.6 Oxalic acid solution (100 g/L). 3.2.7 Sodium hydroxide solution (200 g/L). 3.2.8 Hydrochloric acid (1+1). 3.2.9 Hydrochloric acid (1+4). 3.2.10 Ammonia water (1+1). 3.2.11 EDTA (Ethylene Diamine Tetraacetic Acid) solution (about 0.05 mol/L): Weigh 20 g of EDTA and dissolve it in a small amount of water; transfer it into a 1 000 mL volumetric flask; use water to fix the volume; mix well. 3.2.12 Cresol red indicator (2 g/L): Weigh 0.2 g of cresol red and dissolve it in 100 mL of ethanol solution (1+1). 3.2.13 Phenolphthalein ethanol solution (10 g/L). 3.2.14 Acetic acid-sodium acetate buffer solution (pH 5.5): Weigh 200 g of sodium acetate and dissolve it in a small amount of water; transfer it into a 1 000 mL volumetric flask; add 10 mL of glacial acetic acid (w ≥ 99.5%); use water to fix the volume; mix well. 3.2.15 Xylenol orange indicator (4 g/L): Weigh 0.4 g of xylenol orange and 20 g of potassium nitrate; dissolve in a small amount of water; transfer to a 100 mL volumetric flask; use water to fix the volume; mix well. Store in a brown bottle. 3.2.16 Sodium fluoride solution (40 g/L). 3.2.17 Aluminum standard solution: Weigh 1.000 0 g of metallic aluminum (spectrally pure, remove all surface oxides before use) into a 500 mL beaker; add 50 mL of water; then, add 40 mL of hydrochloric acid (3.2.1); dissolve at low temperature until clear (add hydrochloric acid and water in between); cool. Transfer to a 1 000 mL volumetric flask; use hydrochloric acid (5+95) to dilute to the mark; mix well. This standard solution contains 1 mg of aluminum in 1 mL. 3.2.18 Zinc sulfate solution (about 0.1 mol/L): Weigh 30 g of zinc sulfate (ZnSO4·7H2O) and dissolve it in an appropriate amount of water; transfer it into a 1 000 mL volumetric flask; use water to fix the volume; mix well. 3.2.19 Zinc sulfate standard solution. 3.2.19.1 Preparation: Weigh 2.4 g of zinc sulfate (ZnSO4·7H2O) and dissolve it in a small amount of water; transfer it into a 1 000 mL volumetric flask; use water to fix the volume; mix well. 3.2.19.2 Calibration: Pipette 10.00 mL of aluminum standard solution (3.2.17) into a 250 mL conical flask; add 20 mL of LEDTA solution (3.2.11); add 1 ~ 2 drops of phenolphthalein ethanol solution (3.2.13); use sodium hydroxide solution (3.2.7) to neutralize until red appears. Use hydrochloric acid (3.2.9) to neutralize until colorless and add 1 drop in excess; add 20 mL of acetic acid-sodium acetate buffer solution (3.2.14); boil slightly at low temperature for 1 min ~ 2 min; remove and cool. Perform the following operations according to the analytical steps (3.4.4). Calculate the concentration of zinc sulfate standard solution according to Formula (2): Where: c – concentration of zinc sulfate, in moles per liter (mol/L); ρ0 – mass concentration of aluminum standard solution, in milligrams per milliliter (mg/mL); V1 – volume of aluminum solution pipetted, in milliliters (mL); M – molar mass of aluminum, in grams per mole (g/mol); V2 – volume of zinc sulfate standard solution consumed, in milliliters (mL). 3.3 Test sample 3.3.1 The particle size of the test sample is less than 0.074 mm. 3.3.2 Pre-dry the sample at 105 ℃ ~ 110 ℃ for 2 h; then, place it in a desiccator to cool to room temperature. 3.4 Procedure 3.4.1 Test material Weigh 0.25g of test sample (3.3), accurate to 0.000 1 g. 3.4.2 Time of determinations Independently perform two determinations; take the average value. 3.4.3 Blank test Carry out a blank test together with the test material (3.4.1). 3.4.4 Preparation of analytical solution 3.4.4.1 Place the test material (3.4.1) in a 150 mL polytetrafluoroethylene beaker; add 5 mL of hydrochloric acid (3.2.8) and 1 mL of hydrogen peroxide (3.2.3); heat at low temperature to decompose for 3 min; add 5 mL of hydrofluoric acid (3.2.2) and continue to decompose for 5 min; add 8 mL of perchloric acid (3.2.4) until fuming and evaporate to dryness; remove and cool slightly; add 5 mL of hydrochloric acid (3.2.8) to decompose clearly; transfer to a 200 mL beaker; add 10 mL of hot oxalic acid solution (3.2.6); shake well; add 3 ~ 5 drops of cresol red indicator (3.2.12); use hydrochloric acid (3.2.9) and ammonia water (3.2.10) to adjust to orange-red (pH 1.5 ~ 2.0); keep warm at 40 ℃ for 30 min; cool; transfer the test solution to a 100 mL volumetric flask; dilute to the mark; mix well. 3.4.4.2 Use medium-speed quantitative filter paper to dry-filter the test solution (3.4.4.1) into a 100 mL beaker; transfer 50.00 mL of the solution into a 250 mL conical flask; add 10 mL of nitric acid (3.2.5) and 5 mL of perchloric acid (3.2.4); evaporate at low temperature until all white smoke is emitted; remove and cool; add 5 mL of hydrochloric acid (3.2.8); rinse with a small amount of water; heat slightly until boiling for a few moments to dissolve all the salts. 3.4.4.3 Remove the test solution (3.4.4.2); add 20 mL of EDTA solution (3.2.11); add 1 ~ 2 drops of phenolphthalein ethanol solution (3.2.13); use sodium hydroxide solution (3.2.7) to neutralize until red appears. Use hydrochloric acid (3.2.9) to neutralize until colorless appears and add 1 drop in excess; add 20 mL of acetic acid-sodium acetate buffer solution (3.2.14); boil slightly for 1 min ~ 2 min; remove and cool. 3.4.4.4 Add 2 drops of xylenol orange indicator (3.2.15) to the test solution (3.4.4.3); use zinc sulfate solution (3.2.18) to titrate until it is close to red; then, continue to titrate with zinc sulfate standard solution (3.2.19) until pure red appears (ignore the reading). Add 15 mL of sodium fluoride solution (3.2.16); boil slightly for 1 min ~ 2 min; remove and cool; use zinc sulfate standard solution (3.2.19) to titrate until pure red is the end point. Record the volume of zinc sulfate standard solution (3.2.19) consumed. 3.5 Calculation of analysis result Calculate the mass fraction of aluminum oxide w (Al2O3) according to Formula (3): ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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